EP2631219A1 - Verfahren zur Reduzierung des gesamtorganischen Kohlenstoffs in hypersalinem Wasser - Google Patents

Verfahren zur Reduzierung des gesamtorganischen Kohlenstoffs in hypersalinem Wasser Download PDF

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Publication number
EP2631219A1
EP2631219A1 EP12156586.5A EP12156586A EP2631219A1 EP 2631219 A1 EP2631219 A1 EP 2631219A1 EP 12156586 A EP12156586 A EP 12156586A EP 2631219 A1 EP2631219 A1 EP 2631219A1
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EP
European Patent Office
Prior art keywords
rpm
halophilic
organic carbon
hypersaline
ppm
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP12156586.5A
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English (en)
French (fr)
Inventor
Christoph Herwig
Simon Rittmann
Bettina Lorantfy
Mohammadhadi Jazini
Gerhard Dr. Henssen
Werner Pohl
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ThyssenKrupp Industrial Solutions AG
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ThyssenKrupp Uhde GmbH
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Priority to EP12156586.5A priority Critical patent/EP2631219A1/de
Priority to PCT/EP2013/053487 priority patent/WO2013124375A2/en
Priority to EP13705985.3A priority patent/EP2817263B1/de
Publication of EP2631219A1 publication Critical patent/EP2631219A1/de
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/05—Conductivity or salinity

Definitions

  • the present invention is directed to a method for the reduction of total organic carbon in hypersaline water.
  • Hypersaline solutions are an important raw material for different chemical processes.
  • One of the most important processes worldwide is the electrolysis of sodium chloride solution for the production of chlorine.
  • This membrane based process is feed with saturated sodium chloride solution with a saline content of up to 25 wt.-%. Due to the high sensitivity of the membrane to the impurities, sodium chloride feed stream must be clean enough to avoid the damage of the membrane which affects significant decrease in membrane lifetime and voltage increase.
  • Effluent brines from other industrial processes may be usable as a feed stream to this electro-membrane process. Since effluent brines usually contain high amount of organic carbon, it is necessary to reduce the total organic carbon (TOC) content as much as it is required by the electro-membrane process.
  • TOC total organic carbon
  • the US Patent Application 2011/0180475 is directed to a process for the treatment of wastewater by adding a consortium of isolated halophilic microorganisms capable of biodegrading crude oil in brine.
  • the TOC content of the wastewater varies between 550 mg/l and 600 mg/l.
  • the hydrocarbon content is reduced by a batch fermentation combined with a membrane based process, whereby type and characteristics of the metabolized ingredients is not further differentiated.
  • the wastewater has a salinity of approximately 3,5 wt.-%, which is far away from the requested salinity necessary for the effective electrolysis of sodium chloride solution for the production of chlorine.
  • the underlying problem of the invention is to provide a biological method for the reduction of specific substances as part of the total organic carbon (TOC) in hypersaline solution.
  • the present invention relates to a method for the reduction of total organic carbon in a hypersaline solution, including the following steps:
  • TOC total organic carbon
  • hypersaline solution describes saturated solutions with a high salinity. The solutions are mostly suitable for the production of chlorine in electrolysis.
  • different constituents of the hypersaline solution means all constituents which are necessary to cultivate the added suspension of microorganisms without taking the whole solution. Brine is an industrial product in terms of hypersaline solution and therefore used in parallel to the term "hypersaline solution”.
  • halophilic or "haloalkaliphilic” with respect to the microorganism suspension describes at least one microorganism that is isolated from saline or hypersaline environment and provide as suspension.
  • the suspension can also comprise a consortium of halophilic/haloalkaliphilic microorganisms. These microorganisms are able to metabolize organic carbon, in particular glycerol, in a hypersaline environment.
  • the majority of the TOC content in the hypersaline solution was glycerol (propane-1,2,3-triol), 2,3-epoxy-1-propanol, 2,3-dichlor-1-propanol, moreover, even its derivatives in lower amounts.
  • glycerol also acetates and/or derivates and oligomers are main constituents of the organic carbon content.
  • the hypersaline solution has a salinity of at least ⁇ 15 %, preferably ⁇ 20 %, more preferably ⁇ 25 %. This range is the ideal content when used as feed stream in chlorine production by electrolysis. This saline content can be found in different industrial wastewater.
  • the hypersaline solution is industrial wastewater, preferable brine.
  • the isolated microorganism can be serve a suspension of a single strain or as consortium of different strains cultivated in common. This suspension is added to the hypersaline solution thereby forming a composition of the hypersaline solution and the microorganism.
  • the microorganisms in the microorganism suspension is selected from the group of halophilic strains consisting of Haloferax mediterranei, Halobacterium salinarum and Salinibacter ruber or is selected from the group of haloalkaliphilic strains consisting of Natronomonas pharaoni , Natronobacterium gregoryi , Natronobacterium magadii, Halorubrum vacuolatum, Natronococcus amylolyticus, Natronococcus occultus and Natronorubrum tibetense.
  • the analytic results showed that glycerol; cyclic glycerol and tri-glycerol can be taken up considerably by two of the halophilic strains, Haloferax mediterranei (HFX) and Halobacterium salinarum (NRC).
  • Halobacterium salinarum could only be cultivated on a defined medium, which contains amino acids.
  • Concerning further scale-up issues, the utilization of amino acids in the medium for the strains are difficult to be carried out in industrial scale.
  • the microorganism suspension is based on the halophilic strain Haloferax mediterranei.
  • the hypersaline solution has an initial total organic carbon content (TOC) in the range of 400 ppm to 2500 ppm, preferably 600 ppm to 2500 ppm and a remaining total organic carbon content of less than 100 ppm, preferably less than 50 ppm, more preferably less than 10 ppm.
  • TOC initial total organic carbon content
  • the residual glycerol concentration is also a cornerstone in the method. If the method is carried out as continuous fermentation and the culture residual substrate concentration is not zero in steady-state, the culture is not only limited by the C-source, other limitations are also present.
  • a defined medium is added to the composition provided in step a).
  • This defined medium includes all necessary growth elements for the strains that are not present in the hypersaline solution.
  • the medium is as such a nutrient or culture medium for the strains, chosen before. It can be provided as standard medium with all necessary elements or as reduced medium, e.g. trace elements, in addition to the elements already present in the hypersaline solution.
  • the cultivation has been optimized due to several parameters.
  • the cultivation is based on defined conditions comprising the following fermentation process parameter:
  • the pH range depends on the specific choice of the microorganism strains. For halophilic and/or haloalkaliphilic microorganisms is the pH range from 6,8 to 9,5. The same applies for the cultivation temperature which also depends on the choice of the strains and could vary from 36°C up to 39°C. The selection of the right agitation is affected by the balance between disruption of cells and increase of cell activity in the bioreactor.
  • the air inlet varies in a range of 0,1 to 1,5 vvm (volume gas per volume reactor and minute).
  • the cultivation in step b) leads to a growth rate of the microorganisms that ranges from 0,010 1/h to 0,045 1/h, preferably 0,020 to 0,035 1/h.
  • the exponential growth phase can be characterized by the base consumption, since the exponential curve, which can be fit to the base consumption curve, shows the maximum growth rate ( ⁇ max ) in the batch phase.
  • the method is carried out as batch, fed-batch or continuous fermentation process in a non-corrosive bioreactor.
  • a non-corrosive bioreactor for example a special non-corrosive borsilicate bioreactors is Labfors PEEK by Infors AG, Switzerland.
  • Another aspect of the invention is directed to a medium composition for halophilic microorganisms, preferably Haloferax mediterranei, comprising the following components: Glycerol 1,5 to 10 to g/l, NH 4 Cl 2 g/l, KH 2 PO 4 0,06 to 0,3 g/l, FeCl 3 0,005 g/l, NaCl 194 to 250 g/l, MgCl 2 x 6H 2 O 3,2 to 16 g/l, MgSO 4 x 7H 2 O 4,8 to 24 to g/l, CaCl 2 x 6H 2 O 1 g/l, KCl 5 g/l, NaHCO 3 0,2 g/l, KBr 0,5 g/l, and Trace element solution (Fe, Cu, Mn, Zn) 1 ml.
  • Glycerol 1,5 to 10 to g/l NH 4 Cl 2 g/l, KH 2 PO 4 0,06 to 0,3 g/l, FeCl
  • the medium is as such a synthetic one and can be used for the pre-cultivation of the strains as well as in combination with the hypersaline solution.
  • Ideal growing conditions of halophiles, with Labfors PEEK reactor are given by applying the following parameters:
  • Another aspect of the invention is directed to the mixture of the medium composition and at least one cultured halophilic microorganism suspension, preferably Haloferax mediterranei , and hypersaline brine, wherein the concentration of the brine in relation to the mixture is ⁇ 90 %, preferably ⁇ 75%, more preferably ⁇ 50%.
  • Yet another aspect of the invention is directed to the use of halophilic and/or haloalkaliphilic microorganisms in a method as described above.
  • Example 1 selection of microorganisms
  • the selected microorganisms were cultivated in shake flasks both in their complex as well as defined media and in brine.
  • the strains were cultivated in shake-flasks. Regarding the results of the shake-flask experiments, the analytic results showed that glycerol; cyclic glycerol and tri-glycerol can be taken up considerably by two chosen halophilic strains, Haloferax mediterranei (HFX) and Halobacterium salinarum (NRC). The best defined media and pH ranges were also chosen for both strains for further quantitative studies in bioreactor.
  • HFX Haloferax mediterranei
  • NRC Halobacterium salinarum
  • haloalkaliphilc strains four of them ( Natronomonas pharaonis, Natronococcus occultus, Halorubrum vacuolatum, Natronorubrum tibetense ) were successfully cultivated in defined medium with the carbon source glycerol in shake flasks. Due to the limitations of the shake-flask experiments, e.g. no pH control or no aeration can be done; further consequences could not be drawn. Hence, further study were carried out in bioreactor, which is suitable for cultivations in hypersaline environments and equipped with non-corrosive elements.
  • the strain HFX was chosen to carry out batch and continuous experiments in the bioreactor.
  • the defined medium for the strain HFX was the following (Table 1): Component g/L Glycerol 10 NH 4 Cl 2 KH 2 PO 4 0.3 FeCl 3 0,005 NaCl 194 MgCl 2 .6H 2 O 16 MgSO 4 .7H 2 O 24 CaCl 2 .6H 2 O 1 KCl 5 NaHCO 3 0,2 KBr 0,5 pH 7,2 Trace element solution (Fe, Cu, Mn, Zn) 1mL
  • the defined medium for the haloalkaliphilc strains were as follows (Table 2): Component g/L Glycerol 10 NaCl 198,7 Na 2 CO 3 18,55 KCl 2,01 Na 2 HPO 4 .7H 2 O 0,32 NaH 2 PO 4 .7H 2 O 0,49 MgSO 4 .7H 2 O 0,246 pH 9,2 Trace element solution (Fe, Cu, Mn, Zn) 1mL
  • the aim of the batch experiments was to investigate the feasibility of the cultivation of halophiles on defined medium in the bioreactor.
  • the main markers of growth in the exponential growth phase for instance, the base consumption and the substrate uptake, can be observed ( Fig. 2 and Fig. 3).
  • Fig. 2 shows the characteristics of the substrate uptake in different batch experiments.
  • the exponential growth phase can be characterized by the base consumption, since the exponential curve, which can be fit to the base consumption curve, shows the maximum growth rate ( ⁇ max ) in the batch phase.
  • the exponent of the fitted exponential curve gives estimation to the maximum growth rate ( ⁇ value, 0,043 1/h).
  • agitation was switched from 400 rpm to 500 rpm and to 600 rpm in continuous operation mode.
  • the effects of the agitation change were observed on the activity in the bioreactor.
  • the medium components which were necessary for the microbial growth were added to the brine.
  • the medium composition in Table 1 every inorganic component except NaCl was added.
  • the substrate concentration was completed to 10g/L in the brine, as in the synthetic medium.
  • the glycerol concentration in the feed for the continuous culture was independent from the synthetic:brine feeding ratio and could be considered as constant.
  • the reason for the longer waiting times might be the longer adaptation times of the cells to the brine feed. For example, 5 days were spent with waiting for the steady-state after switching to 20% pre-treated brine, the O 2 signal was constantly increasing and the CO 2 signal was constantly decreasing. Furthermore, according to the optical density analytics of the offline samples, the decreasing turbidity of the bioreactor could be detected. Additionally, the color of the bioreactor was also constantly turning into less reddish.

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  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Biodiversity & Conservation Biology (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Micro-Organisms Or Cultivation Processes Thereof (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Apparatus Associated With Microorganisms And Enzymes (AREA)
EP12156586.5A 2012-02-22 2012-02-22 Verfahren zur Reduzierung des gesamtorganischen Kohlenstoffs in hypersalinem Wasser Withdrawn EP2631219A1 (de)

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Application Number Priority Date Filing Date Title
EP12156586.5A EP2631219A1 (de) 2012-02-22 2012-02-22 Verfahren zur Reduzierung des gesamtorganischen Kohlenstoffs in hypersalinem Wasser
PCT/EP2013/053487 WO2013124375A2 (en) 2012-02-22 2013-02-21 Method for the reduction of total organic carbon in hypersaline water
EP13705985.3A EP2817263B1 (de) 2012-02-22 2013-02-21 Verfahren zur reduzierung des gesamtorganischen kohlenstoffs in hypersalinem wasser

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Cited By (2)

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WO2019170632A1 (en) * 2018-03-09 2019-09-12 Covestro Deutschland Ag Recycling of alkali sulfate rich waste water by biological pre-treatment with an extreme halophilic organism
EP4063331A1 (de) * 2021-03-23 2022-09-28 Covestro Deutschland AG Biologischer abbau von organischen verunreinigungen durch halophile mikroorganismen unter nährstofflimitierung

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JP2019528169A (ja) 2016-08-25 2019-10-10 コベストロ、ドイチュラント、アクチエンゲゼルシャフトＣｏｖｅｓｔｒｏ Ｄｅｕｔｓｃｈｌａｎｄ Ａｇ 耐塩性ハロモナス種（Ｈａｌｏｍｏｎａｓ ｓｐ．）による高塩分環境からのギ酸塩触媒反応
EP3375862A1 (de) 2017-01-10 2018-09-19 Covestro Deutschland AG Biologischer abbau von anilin in hochsalzhaltigen umgebungen unter verwendung von halophilen mikroorganismen
EP3502063A1 (de) * 2017-12-19 2019-06-26 Covestro Deutschland AG Kontinuierliche verfahren zur verminderung der organischen stoffe im abwasser
EP3502065A1 (de) 2017-12-19 2019-06-26 Covestro Deutschland AG Biologischer abbau von organischen schadstoffen durch halophile archaea

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019170632A1 (en) * 2018-03-09 2019-09-12 Covestro Deutschland Ag Recycling of alkali sulfate rich waste water by biological pre-treatment with an extreme halophilic organism
US11530149B2 (en) * 2018-03-09 2022-12-20 Covestro Intellectual Property Gmbh & Co. Kg Recycling of alkali sulfate rich waste water by biological pre-treatment with an extreme halophilic organism
EP4063331A1 (de) * 2021-03-23 2022-09-28 Covestro Deutschland AG Biologischer abbau von organischen verunreinigungen durch halophile mikroorganismen unter nährstofflimitierung
WO2022200019A1 (en) * 2021-03-23 2022-09-29 Covestro Deutschland Ag Biodegradation of organic contaminants by halophilic microorganisms under nutrient limitation
CN116964008A (zh) * 2021-03-23 2023-10-27 科思创德国股份有限公司 营养物限制下嗜盐微生物对有机污染物的生物降解

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WO2013124375A3 (en) 2013-11-21
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EP2817263A2 (de) 2014-12-31

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